反応 #77971

ord-a5c9706326754e45afa5a3da0a92aedc

反応方程式

Oc1cccc2ccccc12
1-naphthol
C1CCC2=NCCCN2CC1
DBU
COc1cccc2ccccc12
1-methoxynaphthalene

反応物

試薬

なし

溶媒

反応条件

温度
90°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度the resulting mixture was heated
  2. 2
    温度The reaction was cooled to ambient temperature
  3. 3
    その他The organic layer was separated
  4. 4
    洗浄washed in sequence with 2M HCl (2×40 mL), 2M NaOH (2×40 mL) and H2O
  5. 5
    乾燥The organic layer was dried over Na2SO4
  6. 6
    ろ過filtered
  7. 7
    濃縮concentrated under vacuum

実験手順

To a solution of 1-naphthol (1.0 g, 6.94 mmol) in DMC (10 mL), DBU (1.06 g, 6.94 mmol) was added and the resulting mixture was heated to reflux (90° C.) for 16 hours. The reaction was cooled to ambient temperature and diluted with EtOAc (50 mL) and H2O (40 mL). The organic layer was separated and washed in sequence with 2M HCl (2×40 mL), 2M NaOH (2×40 mL) and H2O. The organic layer was dried over Na2SO4, filtered and concentrated under vacuum to give 1-methoxynaphthalene as an oil. The yield of 1-methoxynaphthalene as determined by HPLC was 99% conversion.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06706929B2uspto-grants-2004_03